Morpholine → 4-(Morpholin-4-ylmethyl)-1,3-thiazol-2-amine

HRID 1684947

反応式

HRID 1684947 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl.Cl[CH2:9][C:10]1[N:11]=[C:12]([NH2:15])[S:13][CH:14]=1>CN(C=O)C.C(OCC)(=O)C>[O:4]1[CH2:5][CH2:6][N:1]([CH2:9][C:10]2[N:11]=[C:12]([NH2:15])[S:13][CH:14]=2)[CH2:2][CH2:3]1

参加物

5

反応物 2

HCID 8083MorpholineHCID 732282-Thiazolamine, 4-(chloromethyl)-, hydrochloride (1:1)

生成物 1

HCID 21253444-(Morpholin-4-ylmethyl)-1,3-thiazol-2-amine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

Morpholine (350 μL, 4.0.0 mmol) is added to a solution of 4-chloromethyl-thiazol-2-ylamine hydrochloride (368 mg, 2.00 mmol) in DMF (7 mL). The reaction is stirred at 90° C. for 16 h. The reaction is diluted with ethyl acetate and washed with water. The aqueous layer is concentrated in vacuo and extracted with ethyl acetate. The combined organic layers are dried over MgSO4 and evaporated to give brown crystals which are used without further purification. 1H-NMR (400 MHz, d6-DMSO) δ=2.41-2.42 (m, 4H, CH2CH2), 3.30 (s, 2H, CH2), 3.55-3.60 (m, 4H, CH2CH2), 6.33 (s, 1H, Har), 6.85 (bs, 2H, NH2).

後処理

  1. washwashed with water
  2. concentrationThe aqueous layer is concentrated in vacuo
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic layers are dried over MgSO4
  5. customevaporated
  6. customto give brown crystals which
  7. customare used without further purification

出典と根拠

ORDレコード
ord-f5185dbf08d14591b0c720c939f657fc
出典データセット
uspto-grants-2012_04
特許番号
US08148369B2

関連ノート

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